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Herein, guided by the Sabatier principle and Marcus\u2013Hush electron\u2010transfer theory, we report a PyaD COF with dual electronic regulation targeting both atomic active sites and the molecular skeleton. Specifically, moderately polarized active sites balance the adsorption\/desorption step by avoiding overly strong intermediate binding and reducing the H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    desorption barrier from 0.82 to 0.46\u00a0eV, while reinforced interlayer \u03c0\u2013\u03c0 electron coupling across the COF skeleton promotes electron transfer, prolonging the excited\u2010state lifetime by more than one order of magnitude. The dual electronic regulation affords a sacrificial\u2010agent\u2010free H\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    production rate of 4227.5\u00a0\u00b5mol\u00a0g\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    \u00a0h\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>1<\/jats:sup>\n                    , which is approximately 4 times and 2.8 times higher than those of unregulated and singly regulated COFs, respectively. Furthermore, a membrane\u2010based photo\u2010enzyme cascade reactor system achieves selective hydroxylation of ethylbenzene to synthesize 1\u2010phenylethanol, producing over 10\u00a0mmol\u00a0g\n                    <jats:sub>cat<\/jats:sub>\n                    <jats:sup>\u22121<\/jats:sup>\n                    \u00a0L\n                    <jats:sup>\u22121<\/jats:sup>\n                    within five irradiation cycles.\n                  <\/jats:p>","DOI":"10.1002\/anie.5283597","type":"journal-article","created":{"date-parts":[[2026,9,4]],"date-time":"2026-09-04T08:29:21Z","timestamp":1788510561000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Synergic Regulation of Active Site Electron Polarization and Interlayer Electron Coupling in COFs for Photocatalytic Hydrogen Peroxide Synthesis"],"prefix":"10.1002","volume":"65","author":[{"given":"Ruihan","family":"Wang","sequence":"first","affiliation":[{"name":"Joint School of National University of Singapore and Tianjin University International Campus of Tianjin University  Binhai New City, Fuzhou China"},{"name":"Department of Chemical and Biomolecular Engineering National University of Singapore  Singapore Singapore"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4446-6163","authenticated-orcid":false,"given":"Jiafu","family":"Shi","sequence":"additional","affiliation":[{"name":"Joint School of National University of Singapore and Tianjin University International Campus of Tianjin University  Binhai New City, Fuzhou China"},{"name":"State Key Laboratory of Synthetic Biology Tianjin University  Tianjin China"},{"name":"School of Environmental Science and Engineering Tianjin University  Tianjin China"},{"name":"Collaborative Innovation Center of Chemical Science 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